CN115161124A - 一种无腐蚀性的LiF清洗剂及其制备方法 - Google Patents
一种无腐蚀性的LiF清洗剂及其制备方法 Download PDFInfo
- Publication number
- CN115161124A CN115161124A CN202210865028.6A CN202210865028A CN115161124A CN 115161124 A CN115161124 A CN 115161124A CN 202210865028 A CN202210865028 A CN 202210865028A CN 115161124 A CN115161124 A CN 115161124A
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- Prior art keywords
- lif
- cleaning agent
- surfactant
- ethylene glycol
- corrosive
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000012459 cleaning agent Substances 0.000 title claims abstract description 32
- 230000009972 noncorrosive effect Effects 0.000 title claims abstract description 12
- 238000002360 preparation method Methods 0.000 title claims description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 49
- 239000004094 surface-active agent Substances 0.000 claims abstract description 31
- 239000002585 base Substances 0.000 claims abstract description 17
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 12
- 239000002738 chelating agent Substances 0.000 claims abstract description 12
- 239000012498 ultrapure water Substances 0.000 claims abstract description 9
- 239000003513 alkali Substances 0.000 claims abstract description 6
- QIGBRXMKCJKVMJ-UHFFFAOYSA-N Hydroquinone Chemical compound OC1=CC=C(O)C=C1 QIGBRXMKCJKVMJ-UHFFFAOYSA-N 0.000 claims description 22
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims description 15
- QWXYZCJEXYQNEI-OSZHWHEXSA-N intermediate I Chemical compound COC(=O)[C@@]1(C=O)[C@H]2CC=[N+](C\C2=C\C)CCc2c1[nH]c1ccccc21 QWXYZCJEXYQNEI-OSZHWHEXSA-N 0.000 claims description 13
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims description 12
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 11
- 230000015572 biosynthetic process Effects 0.000 claims description 10
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 9
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 9
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 9
- 238000003786 synthesis reaction Methods 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- 238000010992 reflux Methods 0.000 claims description 8
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims description 7
- 239000002202 Polyethylene glycol Substances 0.000 claims description 7
- 150000007529 inorganic bases Chemical class 0.000 claims description 7
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 238000002156 mixing Methods 0.000 claims description 7
- 229920001223 polyethylene glycol Polymers 0.000 claims description 7
- 239000000047 product Substances 0.000 claims description 7
- 239000000243 solution Substances 0.000 claims description 7
- 239000000126 substance Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 6
- WHNWPMSKXPGLAX-UHFFFAOYSA-N N-Vinyl-2-pyrrolidone Chemical compound C=CN1CCCC1=O WHNWPMSKXPGLAX-UHFFFAOYSA-N 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 6
- BWHMMNNQKKPAPP-UHFFFAOYSA-L potassium carbonate Chemical compound [K+].[K+].[O-]C([O-])=O BWHMMNNQKKPAPP-UHFFFAOYSA-L 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 claims description 6
- 239000012043 crude product Substances 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 claims description 4
- AEQDJSLRWYMAQI-UHFFFAOYSA-N 2,3,9,10-tetramethoxy-6,8,13,13a-tetrahydro-5H-isoquinolino[2,1-b]isoquinoline Chemical compound C1CN2CC(C(=C(OC)C=C3)OC)=C3CC2C2=C1C=C(OC)C(OC)=C2 AEQDJSLRWYMAQI-UHFFFAOYSA-N 0.000 claims description 3
- SBASXUCJHJRPEV-UHFFFAOYSA-N 2-(2-methoxyethoxy)ethanol Chemical compound COCCOCCO SBASXUCJHJRPEV-UHFFFAOYSA-N 0.000 claims description 3
- XNWFRZJHXBZDAG-UHFFFAOYSA-N 2-METHOXYETHANOL Chemical compound COCCO XNWFRZJHXBZDAG-UHFFFAOYSA-N 0.000 claims description 3
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 claims description 3
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 claims description 3
- FBPFZTCFMRRESA-FSIIMWSLSA-N D-Glucitol Natural products OC[C@H](O)[C@H](O)[C@@H](O)[C@H](O)CO FBPFZTCFMRRESA-FSIIMWSLSA-N 0.000 claims description 3
- FBPFZTCFMRRESA-JGWLITMVSA-N D-glucitol Chemical compound OC[C@H](O)[C@@H](O)[C@H](O)[C@H](O)CO FBPFZTCFMRRESA-JGWLITMVSA-N 0.000 claims description 3
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims description 3
- 239000004115 Sodium Silicate Substances 0.000 claims description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- XXJWXESWEXIICW-UHFFFAOYSA-N diethylene glycol monoethyl ether Chemical compound CCOCCOCCO XXJWXESWEXIICW-UHFFFAOYSA-N 0.000 claims description 3
- 229940075557 diethylene glycol monoethyl ether Drugs 0.000 claims description 3
- QLBHNVFOQLIYTH-UHFFFAOYSA-L dipotassium;2-[2-[bis(carboxymethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [K+].[K+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O QLBHNVFOQLIYTH-UHFFFAOYSA-L 0.000 claims description 3
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims description 3
- 238000004821 distillation Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 229910000027 potassium carbonate Inorganic materials 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 3
- 238000002390 rotary evaporation Methods 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 239000001509 sodium citrate Substances 0.000 claims description 3
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 3
- 239000000176 sodium gluconate Substances 0.000 claims description 3
- 235000012207 sodium gluconate Nutrition 0.000 claims description 3
- 229940005574 sodium gluconate Drugs 0.000 claims description 3
- 235000019795 sodium metasilicate Nutrition 0.000 claims description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 3
- 239000000600 sorbitol Substances 0.000 claims description 3
- UEUXEKPTXMALOB-UHFFFAOYSA-J tetrasodium;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O UEUXEKPTXMALOB-UHFFFAOYSA-J 0.000 claims description 3
- FYZXEMANQYHCFX-UHFFFAOYSA-K tripotassium;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxymethyl)amino]acetate Chemical compound [K+].[K+].[K+].OC(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O FYZXEMANQYHCFX-UHFFFAOYSA-K 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 abstract description 28
- 238000005260 corrosion Methods 0.000 abstract description 21
- 230000007797 corrosion Effects 0.000 abstract description 21
- 229910003002 lithium salt Inorganic materials 0.000 abstract description 8
- 159000000002 lithium salts Chemical class 0.000 abstract description 8
- 230000003670 easy-to-clean Effects 0.000 abstract 1
- PQXKHYXIUOZZFA-UHFFFAOYSA-M lithium fluoride Chemical compound [Li+].[F-] PQXKHYXIUOZZFA-UHFFFAOYSA-M 0.000 description 42
- 230000000694 effects Effects 0.000 description 21
- 238000000034 method Methods 0.000 description 14
- 238000001704 evaporation Methods 0.000 description 13
- 230000008020 evaporation Effects 0.000 description 13
- 230000000052 comparative effect Effects 0.000 description 11
- 230000008569 process Effects 0.000 description 10
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- 239000000203 mixture Substances 0.000 description 7
- 239000013078 crystal Substances 0.000 description 5
- 230000005764 inhibitory process Effects 0.000 description 5
- 229910052715 tantalum Inorganic materials 0.000 description 5
- GUVRBAGPIYLISA-UHFFFAOYSA-N tantalum atom Chemical compound [Ta] GUVRBAGPIYLISA-UHFFFAOYSA-N 0.000 description 5
- IAZDPXIOMUYVGZ-WFGJKAKNSA-N Dimethyl sulfoxide Chemical compound [2H]C([2H])([2H])S(=O)C([2H])([2H])[2H] IAZDPXIOMUYVGZ-WFGJKAKNSA-N 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 239000007772 electrode material Substances 0.000 description 4
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
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- 239000002184 metal Substances 0.000 description 3
- 229910017604 nitric acid Inorganic materials 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
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- 239000003599 detergent Substances 0.000 description 2
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- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000002244 precipitate Substances 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- 238000007738 vacuum evaporation Methods 0.000 description 2
- QLOKJRIVRGCVIM-UHFFFAOYSA-N 1-[(4-methylsulfanylphenyl)methyl]piperazine Chemical compound C1=CC(SC)=CC=C1CN1CCNCC1 QLOKJRIVRGCVIM-UHFFFAOYSA-N 0.000 description 1
- 229910001111 Fine metal Inorganic materials 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
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- 238000000861 blow drying Methods 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000010406 cathode material Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- ZCDOYSPFYFSLEW-UHFFFAOYSA-N chromate(2-) Chemical compound [O-][Cr]([O-])(=O)=O ZCDOYSPFYFSLEW-UHFFFAOYSA-N 0.000 description 1
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- 125000004430 oxygen atom Chemical group O* 0.000 description 1
- BPUBBGLMJRNUCC-UHFFFAOYSA-N oxygen(2-);tantalum(5+) Chemical compound [O-2].[O-2].[O-2].[O-2].[O-2].[Ta+5].[Ta+5] BPUBBGLMJRNUCC-UHFFFAOYSA-N 0.000 description 1
- 125000002467 phosphate group Chemical group [H]OP(=O)(O[H])O[*] 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
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- 238000006467 substitution reaction Methods 0.000 description 1
- HIFJUMGIHIZEPX-UHFFFAOYSA-N sulfuric acid;sulfur trioxide Chemical compound O=S(=O)=O.OS(O)(=O)=O HIFJUMGIHIZEPX-UHFFFAOYSA-N 0.000 description 1
- PBCFLUZVCVVTBY-UHFFFAOYSA-N tantalum pentoxide Inorganic materials O=[Ta](=O)O[Ta](=O)=O PBCFLUZVCVVTBY-UHFFFAOYSA-N 0.000 description 1
- 238000009210 therapy by ultrasound Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/66—Non-ionic compounds
- C11D1/78—Neutral esters of acids of phosphorus
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic Table
- C07F9/02—Phosphorus compounds
- C07F9/547—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom
- C07F9/553—Heterocyclic compounds, e.g. containing phosphorus as a ring hetero atom having one nitrogen atom as the only ring hetero atom
- C07F9/572—Five-membered rings
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/32—Polymers modified by chemical after-treatment
- C08G65/329—Polymers modified by chemical after-treatment with organic compounds
- C08G65/335—Polymers modified by chemical after-treatment with organic compounds containing phosphorus
- C08G65/3356—Polymers modified by chemical after-treatment with organic compounds containing phosphorus having nitrogen in addition to phosphorus
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- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D1/00—Detergent compositions based essentially on surface-active compounds; Use of these compounds as a detergent
- C11D1/008—Polymeric surface-active agents
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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- C11D3/0005—Other compounding ingredients characterised by their effect
- C11D3/0073—Anticorrosion compositions
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/044—Hydroxides or bases
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/046—Salts
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
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- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/08—Silicates
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/02—Inorganic compounds ; Elemental compounds
- C11D3/04—Water-soluble compounds
- C11D3/10—Carbonates ; Bicarbonates
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/2003—Alcohols; Phenols
- C11D3/2041—Dihydric alcohols
- C11D3/2044—Dihydric alcohols linear
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/20—Organic compounds containing oxygen
- C11D3/2068—Ethers
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D3/00—Other compounding ingredients of detergent compositions covered in group C11D1/00
- C11D3/16—Organic compounds
- C11D3/26—Organic compounds containing nitrogen
- C11D3/33—Amino carboxylic acids
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11D—DETERGENT COMPOSITIONS; USE OF SINGLE SUBSTANCES AS DETERGENTS; SOAP OR SOAP-MAKING; RESIN SOAPS; RECOVERY OF GLYCEROL
- C11D2111/00—Cleaning compositions characterised by the objects to be cleaned; Cleaning compositions characterised by non-standard cleaning or washing processes
- C11D2111/10—Objects to be cleaned
- C11D2111/14—Hard surfaces
- C11D2111/24—Mineral surfaces, e.g. stones, frescoes, plasters, walls or concretes
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- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Wood Science & Technology (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Emergency Medicine (AREA)
- Polymers & Plastics (AREA)
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Abstract
本发明公开了一种无腐蚀性的LiF清洗剂，该清洗剂是由无机碱、螯合剂、有机助剂、表面活性剂及高纯水组成。本发明通过特定的乙二醇基曼尼希碱表面活性剂与无机强碱混配，能提高对锂盐的溶解度，有效解决现有OLED掩膜版及坩埚清洗效率低、对锂盐溶解性差及易造成腐蚀等问题，且其易清洗无残留，具有良好应用前景。
Description
技术领域
本发明属于湿电子化学品领域，具体涉及一种无腐蚀的用于清洗LiF材料的清洗剂，其能快速并有效的清洗去除蒸镀工艺中掩膜版及坩埚上附着的氟化锂电极材料，并具有易清洗、无残留，且对清洗部件无腐蚀等优势，可有效提高掩膜版及坩埚的清洗效率。
背景技术
在OLED显示器制造工艺中比较成熟的是OLED蒸镀技术。蒸镀技术需要精密的蒸镀设备，以及用于蒸镀的精细金属掩膜版（FMM）。在重复的蒸镀过程中，阴极材料氟化锂会在FMM和坩埚上沉积，造成堵塞与污染，严重影响后续蒸镀的效果。因此在生产时，坩埚和FMM都需要定期进行清洗，来确保其后续效能。
OLED坩埚作为OLED生产过程中的核心蒸镀单元，本身需要具备很高的耐温性和热稳定性，尤其是在LiF薄膜的真空蒸镀过程中，加热到一定程度后坩埚内部的材料会在熔化后的冷却过程中形成坚硬的结晶体结构，并与坩埚内壁紧密的粘结在一起，普通清洗剂很难将其溶解或使其与坩埚本体分离。
坩埚焊接材料的材质为钽。钽具有低蒸汽压、低蒸发速率、低韧脆转变温度、耐腐蚀性极好、特殊的介电性能等特点；钽的抗腐蚀性很强，是由于表面可生成稳定的五氧化二钽（Ta2O5）保护膜。但钽在游离的SO3或SO2的发烟硫酸、氟气、氢氟酸及含氟离子超过10ppm的溶液中会发生腐蚀，热的NaOH、KOH溶液会腐蚀钽，并导致氢脆。
传统的坩埚和FMM上电极材料的清洗主要采用酸洗，其不仅具有很强的腐蚀性，而且产生的废酸难以处理，污染环境，并造成了OLED显示器制备成本的提高。专利CN111501085A公开了真空蒸镀设备中Mask的清洗方法，其是以硝酸溶液为电解液，以待清洗Mask作为阳极，通过与电源负极连接使Mask表面的金属膜溶解于硝酸电解液而达到清洗效果。专利CN 112718692A公开了一种坩埚部品LiF结晶物的清洗方法，其是通过将浓盐酸与浓硝酸按1:1混合后，将混合药液置于超声波槽体中，将待清洗的坩埚部品放置于超声波处中浸泡6h-8h直到LiF材料电解出F-且坩埚部品表面出现色差停止浸泡，采用百洁布打磨或采用G400#砂材喷砂的方式去除经浸泡的坩埚部品表面的结晶体，完成对坩埚部品LiF结晶物的清洗。但采用酸洗的方式对设备的腐蚀性强，产生的废酸污染环境，废液处理成本高。而目前市面上采用碱洗的方式，往往都存在清洗效率低、清洗效果差、对锂盐的溶解性低、器件腐蚀、寿命低等问题。
发明内容
本发明的目的是提供一种无腐蚀性的LiF清洗剂，其通过添加特定的乙二醇基曼尼希碱表面活性剂，大大提高了清洗剂对锂盐的溶解度，可以快速并有效去除蒸镀工艺中掩膜版及蒸镀设备坩埚上附着的LiF电极材料，从而有效提高了清洗效率，并可同时解决清洗过程中产生腐蚀的问题。
为实现上述目的，本发明采用如下技术方案：
一种无腐蚀性的LiF清洗剂，按质量百分数之和为100%计，其所用各原料及各原料所占质量百分数为：
无机碱 5-15%，
螯合剂 1-5%，
有机助剂 1-5%，
表面活性剂 0.1-5%，
余量为高纯水。
其中，所述无机碱为氢氧化钾、氢氧化钠、碳酸钠、碳酸钾、偏硅酸钠中的一种或多种。
所述螯合剂为葡萄糖酸钠、乙二胺四乙酸、乙二胺四乙酸二钠、乙二胺四乙酸四钠、乙二胺四乙酸二钾、乙二胺四乙酸三钾、柠檬酸、柠檬酸钠、山梨糖醇中的一种或多种。
所述有机助剂为乙醇、乙二醇、丙二醇、乙二醇甲醚、乙二醇乙醚、乙二醇丁醚、二乙二醇单甲醚、二乙二醇单乙醚中的一种或多种。
所述高纯水25℃时的电导率不低于18MΩ的去离子水。
所述表面活性剂为乙二醇基曼尼希碱表面活性剂，其化学结构式为：
（1）中间体Ⅰ的合成
将N-乙烯吡咯烷酮和甲醛混合后，加入一定量对苯二酚，然后将混合液转移至带有回流装置的三口烧瓶中，通入N2约30min以除去反应体系中的氧气，再升温至90℃，并用恒压分液漏斗向其中缓慢滴加苯胺，滴加完毕后升温到140 ℃反应6h，即得到中间体Ⅰ，其化学结构式为：
；其中，N-乙烯吡咯烷酮、甲醛、对苯二酚及苯胺的摩尔比为1.2:1.2:1.0:1.0；
（2）中间体Ⅱ的合成
在所得中间体Ⅰ中加入甲醛、亚磷酸混匀，并加入一定量的对苯二酚，在装有冷凝回流装置的三口烧瓶中90℃回流7h，得到中间体Ⅱ，其化学结构式为：
（3）乙二醇基曼尼希碱表面活性剂的合成
将中间体Ⅱ和聚乙二醇按摩尔比1:1在无溶剂条件下130℃蒸馏反应6h，反应完的粗产物先用去离子水洗涤2次，再用甲醇水混合液（甲醇/水=4:1，v/v）洗涤一次，洗涤完的产物溶解在氯仿中，经无水硫酸钠干燥后旋蒸即得。
进一步地，所述LiF清洗剂的制备方法是往高纯水中先添加无机碱、有机助剂，然后加入表面活性剂，在500rpm的转速下搅拌使其形成均一体系，再一边搅拌一边加入螯合剂，以最终得到均一稳定澄清透明的溶液。
本发明的有益效果为：
（1）本发明通过无机强碱性物质和有机碱的相互作用，可以将MASK和坩埚上残留的氟化锂剥离下来，且乙二醇基曼尼希碱表面活性剂的使用，不仅可极大程度上提高体系的表面活性，由于聚乙二醇是直链结构，Li+可对其链节上的氧原子产生诱导，使聚乙二醇的链节形成半交叉式构象重叠式螺旋结构并与Li+络合，从而可起到增溶LiF的作用，即可使不溶性的LiF转化为可溶性的锂盐。
（2）本发明所采用的特定的乙二醇基曼尼希碱表面活性剂具有较好的耐碱性能，且其在金属表面活性位点具有成膜效应，可使得腐蚀介质不能与金属直接接触，从而达到较好的缓蚀效果，同时，其在金属表面形成的保护膜，可消除腐蚀性离子，阻止金属的氧化和电子的产生，并可防止氧气运输到金属表面，这也有效的阻碍了阳极和阴极反应，极大的减缓了腐蚀进程。此外，其结构中亚磷酸基团的引入，增加了曼尼希碱在腐蚀介质中的分散性与缓蚀性能。
（3）本发明提供的LiF清洁剂克服了现有碱洗工艺中存在的清洗效率低、对锂盐溶解性低，且对坩埚器件产生腐蚀等问题，可以有效降低MASK和坩埚的清洗成本，提高对锂盐的溶解度，同时解决了清洗过程中的腐蚀问题。
附图说明
图1为使用实施例1清洗剂清洗前后坩埚的效果对比图，a为清洗前，b为清洗后。由图可以看出，其清洗效果符合要求，无沉淀产生，无腐蚀现象产生。
图2为使用对比例4清洗剂浸泡前后坩埚的效果对比图，a为浸泡前，b为浸泡后。由图可以看出，坩埚表面发黑，但无沉淀产生，清洗效果满足要求。
图3为使用对比例5清洗剂浸泡前后坩埚的效果对比图，a为浸泡前，b为浸泡后。由图可以看出，坩埚表面有白色粉末产生。
图4为实施例1及对比例4、5、6浸泡7天后的电化学测试的阻抗图。由图可以看出，添加特定乙二醇基曼尼希碱表面活性剂缓蚀效果显著（阻抗越大，缓蚀效果越好）。
具体实施方式
一种无腐蚀性的LiF清洗剂，按质量百分数之和为100%计，其所用各原料及各原料所占质量百分数为：
无机碱 5-15%，
螯合剂 1-5%，
有机助剂 1-5%，
表面活性剂 0.1-5%，
余量为高纯水。
所述LiF清洗剂的制备方法是往高纯水中先添加无机碱、有机助剂，然后加入表面活性剂，在500rpm的转速下搅拌使其形成均一体系，再一边搅拌一边加入螯合剂，以最终得到均一稳定澄清透明的溶液。
其中，所述无机碱为氢氧化钾、氢氧化钠、碳酸钠、碳酸钾、偏硅酸钠中的一种或多种。
所述螯合剂为葡萄糖酸钠、乙二胺四乙酸（EDTA）、乙二胺四乙酸二钠、乙二胺四乙酸四钠、乙二胺四乙酸二钾、乙二胺四乙酸三钾、柠檬酸、柠檬酸钠、山梨糖醇中的一种或多种。
所述有机助剂为乙醇、乙二醇、丙二醇、乙二醇甲醚、乙二醇乙醚、乙二醇丁醚、二乙二醇单甲醚、二乙二醇单乙醚中的一种或多种。
所述高纯水25℃时的电导率不低于18MΩ的去离子水。
所述表面活性剂为乙二醇基曼尼希碱表面活性剂，其化学结构式为：
（1）中间体Ⅰ的合成
将N-乙烯吡咯烷酮和甲醛混合后，加入一定量对苯二酚，然后将混合液转移至带有回流装置的三口烧瓶中，通入N2约30min以除去反应体系中的氧气，再升温至90℃，并用恒压分液漏斗向其中缓慢滴加苯胺，滴加完毕后升温到140 ℃反应6h，即得到中间体Ⅰ；其中，N-乙烯吡咯烷酮、甲醛、对苯二酚及苯胺的摩尔比为1.2:1.2:1.0:1.0；
（2）中间体Ⅱ的合成
在所得中间体Ⅰ中加入甲醛、亚磷酸混匀，并加入一定量的对苯二酚，在装有冷凝回流装置的三口烧瓶中90℃回流7h，得到中间体Ⅱ；其中，中间体Ⅰ与甲醛、亚磷酸、对苯二酚的摩尔比为1:1:0.9:1；
（3）乙二醇基曼尼希碱表面活性剂的合成
将中间体Ⅱ和聚乙二醇按摩尔比1:1在无溶剂条件下130℃蒸馏反应6h，反应完的粗产物先用200ml去离子水洗涤2次，再用100ml甲醇水混合液（甲醇80ml，水20ml）洗涤一次，洗涤完的产物溶解在氯仿中，经无水硫酸钠干燥后旋蒸即得。
当n=2时，所得乙二醇基曼尼希碱表面活性剂的表征数据如下：
1H NMR(300MHz,DMSO-d6),δ: 5.88（d,1H,CH）,5.26（d,1H,CH）,6.96（s,1H,CH）,3.24-3.34（t,2H,CH2），1.86-2.12（m,2H,CH2），2.65（m,1H,CH），3.19-3.44（q,2H,CH2），6.80（m,1H,ArH）,6.94（m,2H,ArH）,7.21（m,2H,ArH），3.70（m,8H,CH2-CH2-O）,3.74（d,2H,CH2）,4.80（s,1H,OH）,5.4（s,1H,OH）。13C NMR(125MHz,DMSO-d6),δ:93.1,147.3,55.0,61.1,35.9,31.8,46.3,138.8,104.7,105.8,15.2,66.6,70.0,61.3。HRMS计算值C18H27O6N2P (M+H)+: 398.16，实测值398.40。
为了使本发明所述的内容更加便于理解，下面结合具体实施方式对本发明所述的技术方案做进一步的说明，但是本发明不仅限于此。
按表1配方配制不同组成的清洗剂组合物。
表1 不同清洗剂组合物中各组分及其含量
将坩埚分别浸泡在实施例1-6和对比例1-6制备的清洗剂组合物中，在40±5℃、40KHZ条件下超声2h，取出后用去离子水清洗，吹干，利用肉眼观察坩埚表面的清洗效果；再将坩埚重新分别浸泡在实施例1-6和对比例1-6制备的清洗剂组合物中，40±5℃浸泡7天后，通过电化学工作站测试及肉眼观察坩埚表面腐蚀情况。结果见表2。
表2 不同清洗剂组合物对坩埚的清洗效果
由表2可以看出，实施例制备的LiF清洗剂均一稳定，并可以将坩埚清洗干净，其无沉淀产生，无腐蚀现象产生，其清洗效果良好。
而与实施例1相比，对比例1提高了无机碱的比例，在操作温度下，其所得清洗剂体系均一稳定，可以快速将坩埚清洗干净，但清洗过程杯底有大量沉淀产生。对比例2不含有机助剂，在操作温度下，无法将坩埚清洗干净。对比例3不含螯合剂，在操作温度下，其所得清洗剂体系均一稳定，但无法在限定时间内将坩埚清洗干净。对比例4不含表面活性剂，在操作条件下，其所得清洗剂体系均一稳定，可以将坩埚清洗干净，但坩埚表面出现腐蚀现象。对比例5用铬酸钾作为表面活性剂，在操作温度下，所得清洗剂体系均一稳定，可以将坩埚清洗干净，坩埚表面无腐蚀现象，但有白色粉末产生，这可能是因为铬酸盐属于无机盐型缓蚀剂，会在坩埚表面形成一层致密的氧化膜。对比例6用苯并咪唑-N-曼尼希碱作为表面活性剂，在操作温度下，所得清洗剂体系均一稳定，可以将坩埚清洗干净，且对坩埚表面无腐蚀现象，但是会产生沉淀现象，这可能是由于其对LiF没有溶解作用。
由上述可以说明，本发明LiF清洗剂中有机助剂具有一定的助漂洗作用，螯合剂具有一定的分散作用，乙二醇基曼尼希碱表面活性剂提高了体系的表面活性，并提高了对锂盐的溶解度，且具有较好的缓蚀性能，因而能使所得清洗剂对蒸镀工艺中掩膜版及蒸镀设备坩埚上附着的LiF电极材料达到良好的清洗效果，其各成分缺一不可。
上述实施例对本发明进行了详细描述，但其只是作为范例，并非因此限制本发明的专利范围。凡是利用本发明说明书对本发明进行的等同任何修改和替代也都在本发明的范畴之中，均包括在本发明的专利保护范围内。
Claims (8)
1.一种无腐蚀性的LiF清洗剂，其特征在于，按质量百分数之和为100%计，所用各原料及其所占质量百分数为：
无机碱 5-15%，
螯合剂 1-5%，
有机助剂 1-5%，
表面活性剂 0.1-5%，
余量为高纯水。
2.根据权利要求1所述的一种无腐蚀性的LiF清洗剂，其特征在于，所述无机碱为氢氧化钾、氢氧化钠、碳酸钠、碳酸钾、偏硅酸钠中的一种或多种。
3.根据权利要求1所述的一种无腐蚀性的LiF清洗剂，其特征在于，所述螯合剂为葡萄糖酸钠、乙二胺四乙酸、乙二胺四乙酸二钠、乙二胺四乙酸四钠、乙二胺四乙酸二钾、乙二胺四乙酸三钾、柠檬酸、柠檬酸钠、山梨糖醇中的一种或多种。
4.根据权利要求1所述的一种无腐蚀性的LiF清洗剂，其特征在于，所述有机助剂为乙醇、乙二醇、丙二醇、乙二醇甲醚、乙二醇乙醚、乙二醇丁醚、二乙二醇单甲醚、二乙二醇单乙醚中的一种或多种。
5.根据权利要求1所述的一种无腐蚀性的LiF清洗剂，其特征在于，所述表面活性剂为乙二醇基曼尼希碱表面活性剂，其化学结构式为：
6. 根据权利要求5所述的一种无腐蚀性的LiF清洗剂，其特征在于，所述表面活性剂的制备方法包括以下步骤：
（1）中间体Ⅰ的合成
将N-乙烯吡咯烷酮和甲醛混合后，加入一定量对苯二酚，然后将混合液转移至带有回流装置的三口烧瓶中，通入N2 30min以除去反应体系中的氧气，再升温至90℃，向其中缓慢滴加苯胺，滴加完毕后升温到140 ℃反应6h，即得到中间体Ⅰ；
（2）中间体Ⅱ的合成
在所得中间体Ⅰ中加入甲醛、亚磷酸混匀，并加入一定量的对苯二酚，90℃下回流反应7ｈ，得到中间体Ⅱ；
（3）表面活性剂的合成
将中间体Ⅱ和聚乙二醇在无溶剂条件下130℃蒸馏反应6h，反应完的粗产物先用去离子水洗涤2次，再用甲醇水混合液洗涤一次，洗涤完的产物溶解在氯仿中，经无水硫酸钠干燥后旋蒸即得。
7.根据权利要求6所述的一种无腐蚀性的LiF清洗剂，其特征在于，步骤（1）中所用N-乙烯吡咯烷酮、甲醛、对苯二酚及苯胺的摩尔比为1.2:1.2:1.0:1.0；
步骤（2）中所用中间体Ⅰ与甲醛、亚磷酸、对苯二酚的摩尔比为1:1:0.9:1；
步骤（3）中所用中间体Ⅱ和聚乙二醇的摩尔比为1:1；所述甲醇水混合液中甲醇与水的体积比为4:1。
8.根据权利要求1所述的一种无腐蚀性的LiF清洗剂，其特征在于，其制备方法是往高纯水中先添加无机碱、有机助剂，然后加入表面活性剂，在500rpm的转速下搅拌使其形成均一体系，再一边搅拌一边加入螯合剂，以最终得到均一稳定澄清透明的溶液。
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